1,2-Dichloroethane → HCID 58333608、化合物

HRID 2066848ノート

反応式

HRID 2066848 の反応式
[CH:1]([O:4][C:5]([N:7]1[CH2:12][CH2:11][CH:10]([O:13][N:14]=[C:15]2[CH2:20][CH2:19][N:18]([C:21]3[CH:26]=[C:25]([F:27])[C:24]([C:28]([OH:30])=O)=[CH:23][C:22]=3[F:31])[CH2:17][CH2:16]2)[CH2:9][CH2:8]1)=[O:6])([CH3:3])[CH3:2].[CH3:32][NH:33][CH3:34].C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl>C(Cl)Cl>[CH:1]([O:4][C:5]([N:7]1[CH2:8][CH2:9][CH:10]([O:13][N:14]=[C:15]2[CH2:20][CH2:19][N:18]([C:21]3[CH:26]=[C:25]([F:27])[C:24]([C:28](=[O:30])[N:33]([CH3:34])[CH3:32])=[CH:23][C:22]=3[F:31])[CH2:17][CH2:16]2)[CH2:11][CH2:12]1)=[O:6])([CH3:3])[CH3:2]

参加物

6

反応物 4

HCID 111,2-DichloroethaneHCID 674DimethylamineHCID 757711-HydroxybenzotriazoleHCID 58333593HCID 58333593、化合物

生成物 1

HCID 58333608HCID 58333608、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

9-1 (30 mg, 0.071 mmol), dimethylamine (0.1 mmol) and HOBT (0.2 mmol) were combined in DCM (1 mL) and stirred at room temperature for 10 minutes. EDC(0.2 mmol) was added and the mixture was stirred for 18 h. The solution was washed with 2 mL of aqueous NaHCO3, concentrated, taken up with 1 mL of methanol and purified on preparative HPLC to give 29-1: LC-MS 467.4 (MH).

後処理

  1. stirringthe mixture was stirred for 18 h
  2. washThe solution was washed with 2 mL of aqueous NaHCO3
  3. concentrationconcentrated
  4. custompurified on preparative HPLC
  5. customto give 29-1

出典と根拠

ORDレコード
ord-d5579f41056b452ebc62ec00f75f7468
出典データセット
uspto-grants-2012_10
特許番号
US08293729B2

反応ノート

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